Composition of matter for flameproofing cellulosic media and method of making the same



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PRQGFKNG SEILULDSIC IVE'EHUD OF G S Frederick W. Hochstetter, Pittsburgh, Pa... assignor to Hochstcttcr Research Laboratories, En'c" Pittsburgh, Pa", a. corporation of Peylvsnis No Brewing. Application Novemher 3, 1941, Serial No. 417.7%

(on. its-i5) it Claims.

My present invention relates to the art of fiameproofing; more particularly, to a. composition of matter for fismeproofing cellulosic or ligno-cellulosic media. or products fabricated therefrom as well as to a. method for producing such composition The art of fiemeprooflng is exceedingly old and well known. y proposals have been made in the prior patents and literature for importing flameproof or fireproof characteristics to cellulose and cellulosic materials. It is widely recognized, however, that all proposedformulss are defective or deficient in one or more particulers. Many of them give of? noxious 'fumes and merely act to retard combustion; others are expensive, diiucult to make or apply and effective,

if at all, only for a. limited period; still others permit'ofter-glow and give off large quantities ,oikv smoke. There is, so far as I am aware, no known eproofing composition which really meets commercial requirements satisfactorily and which will not dissdventegeously afiect the ma.- terisls treated. The desirability and need for on eflective composition that will reduce fire hazards end losses, decrease insurance rates, etc. is, of course, obvious.

It is, accordingly, one of the objects of my present invention to produce a. fismeprooflng composition of matter which will obviate the defects I and disadvantages of known compositions.

Another ob ect of my invention is to produce a composition capable of imparting adequate.

flameprooi characteristics to celldlosic media. and products both in the form of pulpsnd fibres or semi-finished and finished materials;

A fln'therobject of my invention resides in a. compomtion which, when applied to cellulosic materials, shall render the same fiameproof, re-

taining its flameproof characteristics even under unusually high temperature. conditions and even after repeated washings.

7 Materials treated with my new composition do not give so appreciable smoke and are free from otter-glow both during and subsequent to sub- Jectiontoe flame or fire; they do not support combustion but-will, at most, merely char; such constitute further objects of my invention More specifically, my invention includes the useof hexamethylenetetramine and/or salige'nin in combination in a. flameprooflng composition.

A still further object includes procedure for mkingmy, new composition.

L Other andmrther objects and advantages be lindel'stood by those skilled in this art or'will 'be spporent or pointed out hereinafter.

. My present invention is based upon the dismethylenetetramlne, the fiameprooflng charac teristics of the composition are so improved or altered that the media. or products treated therewith can be subjected to repeated washings without loss of flameprooiing quality. Flameproofed products can thus he produced which are wsshproof and non-leaching.

In o. composition for flameproofing which contoms both hexsmethylenetetrsmine and railsenin, in accordance with my present invention, I believe that there is a compound precipitated in or upon the cellulose of the medium orprodnot treated therewith which is in the nature of a.

polymer or partial condensation product, chemically short of a solid end-product, which is perman'ent and non-hardening and which eirectively resists repeated washings, probably also being resistant to the solvent action of water as well as to soaps, washing compounds and the like. In

combination withthe other hereinafter specified ingredients of my new composition, which may take a number of specific forms, 'an unusually eilicacious flameprooflng'is achieved which is far superior to results hitherto attained as indicated by extensive tests and investigations made by me.

The following exemplary formulas have been 'found. by me to achieve the objects and advantagesherein set forth."

Example 1 Parts by weight Aqueous protein (1-10%) About Hexamethylenetetramine About 1-10 Sulphuric acid (-66%) -.About 1-20 Aqueous ammonia (28%) --'About 3-60 Phosphoric acid (commercial) About 1-19 '6 Example 2 1100 parts 1-10 m mom nous motterto y isht 5-10 parts phosphoric acid (commercial) in 100 parts water by weight Example-31b1,! weight) In preparing the composition of Example 1,

.the ingredients are added in the order given rollowing'thetemperatures prescribed in connection with Example 2, so far as applicable. The aqueous protein extract may be prepared by,adding protein to water which has been boiling for about both primary andsecondary reaction products oia complex nature, the resultant composition acting to impart all the above desired characteri's'tics to'cellulosic media and products I n compounding Example 2, the desired amount of water is boiled for about minutes and casein, glue or gelatine added. When casein and scope of the invention. in one-or another isusedit .isiflrst dissolved in the ammonia inascacco of its forms my composition is widely applicable to celiulosic media and products in which flameproofing characteristics are desired. Such may, for example, include mattresses, pillows, cushions and upholstery of various kinds, both the cotton or fibrous fillers and the coverings or tickings thereof; insulating materials such as are used m automobiles and airplanes; clothing, rugs, curtains, draperies, linens and many other materials- The invention may be used to treat the pulp or fibres prior to the making up of media and products therefrom.

V I have further discovered that the incorporation of hexamethylenetetramine and/or saligenin in known flameprooiing compositions great- 1y improves the effectiveness of such compositions to a marked extent.

What I claim is:

1. An aqueous composition of matter or the character described, which is capable of convetting infl f' able celiulosic materials to a non-inflammable condition and which is essentially composed of the reaction product of hexamethylenetetramine 'and oxybenzylalcohol.

2. A j ,washproof and non-leaching, non-combustible; and non-inflammable cellulosic article 'of commerce which is composed of a cellulosic material normally combustible and inflammable,

' Parts Water 10o Nitrogenous matter (derived from. casein or animal colloid) -4 ii -10 Sulphuric acid (66%)-.....' 5-25 Ammonia (aqua) (20%); 15-50 Phosphoric acid (commercial) 5-.10 Hexamethylenetetramine 1-5v Aqueous saiigenin (saturated solution)" 14 Example 4 (by weight)' 2% aqueous solution of animal colloid 100 Ammonium sulphate ..j. 5-10 -Ammonium phosphate 1-5.

Ammonium carbonate '1-5" Borax V 1-5 Boris acid 7 1-5 Hexamethylenetetramine' 1-10 20 minutes. The ingredients interact to form gredient. when glue' or gelatine is used it a 10? iparts by weight of water containing 1-10 parts proe I flrst'softened in cold water and finally cooked for twenty minutes. As soon as the ammonia is addedto-the casein and stirred in a closed vessel the phosphoric acid constituent is added slowly until -a syrupy condition is reached.

the aqueous nitrogenousconstitu'ent at a temperature of about F. is-added and thoroughly 'I'hereupon About 5-25 parts of stirred and then the sulphuric acid added slowly while preventing the temperature from rising above-about'60"F.-. Finally, the hexamethylene- 1 tetramine is added and the temperature gradually-raised-to about.120 F or above if necessaryto keep the mixture fluid.

- Examples 3 and '4 are compounded as per Example-1.

r In connection vention adjustment maybe made so that the composition as, a whole is alkaline, neutral or- ,acid. I' have discovered that this .fleiribility' is important because yarious media and products can-only be-adequately'fiameproofed by compowith all formulas under this incombined with the products of reaction of hexamethylenetetramine and oxybenzylalcohol to Y About 1-10 parts by weight of hexamethylenetetramine;

dilute protein extract About 1-20 parts by weight of 66% sulphuric acid;

Aboug 3-60 parts'by weight 0! 28% aqueous ammonia;

an r

Aboutl 1-10 parts by weight .of commercial phosphoric 4. A flameprooiing composition of matter consisting of the reaction products and unreacted residue of:

n a v About 1-10 parts of hexamethylenetetramine in 100 parts by weight of water;

66 sulphuric acid in 60 parts of water, by weight;

About 15-65 parts of ammonia (28%) in 60-100 parts of water. by weight pnd About 5-10 parts of commercial phosphoric acid in 100 parts of water,,by weight.

' 1-5 parts hexamethylen'etetramine and 1-2 parts orybonzylalcohol.

'8. A flameprooflng composition of matter consisting '01 the reaction products and unreacted residues of:

subjoined claims. "other variations and modidcations maybe resorted to within'-the spirit parts 2% aqueous gelatine extract; 5-10" parts ammonium sulphate 1-5 parts ammonium phosphate; 1-5 parts ammonium carbonate: 1-5 parts how;

1-5 parts Doric-acid: and

1-10 parts hexamethylenete tramine.

7. method ofimaking a flameproonng composition comprising adding 1-10 parts casein to 15-65mm: aquaammonia, mixing the same with water-out of contact with theair, adding 5-10 phosphoric acid. adding 6-25 Da centmted sulphuric acid while preventing a. tem- 8. A method in accordance with c 7 wherein casein is replaced by equivalent amounts of glue or geiatine which has been previously softened in cold water and cooked for about twenty utes.

9. A composition of matter for flameproofing ceiiulosic media. which contains an appreciable proportion of a, semi-solid condensation product of hexamethylene tetramine and oxybenzylalcoho].

FREDERICK W. HOCHSTEI'IEB. 

